Ethyl isocyanate → HCID 135948879, compound

Participants

Reaction Steps

To a solution of EXAMPLE 8A (1.05 g, 4.22 mmol) in pyridine (10 mL) was added ethyl isocyanate (1.0 mL, 12.68 mmol) and the solution heated at reflux overnight. The mixture was cooled, stirred with 15 mL ethyl acetate at ambient temperature for 5 minutes and the solid collected by filtration, washed with ethyl acetate and dried to give 793 mg of the title compound. The mother liquor was concentrated and the residue recrystallized from ethyl acetate to give an additional 300 mg of the title compound (94% overall yield). 1H NMR (DMSO-d6) 1.64-1.75 (m, 4H), 2.16 (s, 6H), 2.34-2.39 (m, 5H), 2.59 (t, J=6.4 Hz, 2H), 2.83-2.87 (m, 2H), 4.18 (t, J=6.6 Hz, 2H).

Provenance & Evidence